Hydrochloric Acid → 6H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro-

HRID 275085

Reaktionsgleichung

[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[OH:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[P:14](Cl)(Cl)[Cl:15].Cl>[Cl-].[Zn+2].[Cl-]>[Cl:15][P:14]1[C:6]2[CH:5]=[CH:4][CH:3]=[CH:2][C:1]=2[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[O:13]1

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

700 g (4.12 mol) of o-phenylphenol and 4.1 g of zinc chloride are heated to 180° C. with stirring. 692 g (5.03 mol) of phosphorus trichloride are then added dropwise over 12 hours. Reflux is maintained for a further 5 hours; at the end no further hydrogen chloride is evolved. The excess phosphorus trichloride is distilled off at 120° C. in vacuo, the reaction product is cooled to 100° C. and 966 g of toluene are added. Cooling to room temperature gives a 50% strength solution of 6-chloro-(6H)-dibenz[c,e][1,2]oxaphosphorin in toluene. The 31P-NMR spectrum indicates a purity of 95.5%.

Aufarbeitung

temperatureReflux
temperatureis maintained for a further 5 hours
distillationThe excess phosphorus trichloride is distilled off at 120° C. in vacuo
addition966 g of toluene are added
temperatureCooling to room temperature

Quellen und Nachweise

ORD-Eintrag: ord-2f7c158a840b4861ba752948915936b2
Quelldatensatz: uspto-grants-1995_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05391798

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